CN107742545A - The preparation method of resin graphene metallic composite - Google Patents

The preparation method of resin graphene metallic composite Download PDF

Info

Publication number
CN107742545A
CN107742545A CN201710968900.9A CN201710968900A CN107742545A CN 107742545 A CN107742545 A CN 107742545A CN 201710968900 A CN201710968900 A CN 201710968900A CN 107742545 A CN107742545 A CN 107742545A
Authority
CN
China
Prior art keywords
graphene
resin
metallic composite
electrode material
deposition
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201710968900.9A
Other languages
Chinese (zh)
Other versions
CN107742545B (en
Inventor
邵光伟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangdong Luhua New Material Technology Holding Co ltd
Original Assignee
Foshan Huichuang Zhengyuan New Mstar Technology Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Foshan Huichuang Zhengyuan New Mstar Technology Ltd filed Critical Foshan Huichuang Zhengyuan New Mstar Technology Ltd
Priority to CN201710968900.9A priority Critical patent/CN107742545B/en
Publication of CN107742545A publication Critical patent/CN107742545A/en
Application granted granted Critical
Publication of CN107742545B publication Critical patent/CN107742545B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20Conductive material dispersed in non-conductive organic material
    • H01B1/22Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20Conductive material dispersed in non-conductive organic material
    • H01B1/24Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables

Abstract

The invention discloses the preparation method of resin graphene metallic composite, the technology utilization oxidation reaction prepares graphene oxide solution, resin dispersion liquid is obtained using ultrasonic disperse microwave treatment, then carrying out electro-deposition by high precision DC power supply obtains resin graphene metallic composite.The resin graphene metallic composite being prepared, its electric property is excellent, electric conductivity is sensitive, has preferable application prospect.

Description

The preparation method of resin graphene metallic composite
Technical field
The present invention relates to this technical field of material, the preparation side of resin graphene metallic composite is related specifically to Method.
Background technology
Traditionally electric conductivity graphene film is by mechanically pulling off to produce.By property, graphite surface is hydrophobic. The oxidation and subsequent stripping of graphite have shown that and produce more soluble graphene oxide, but have relatively low conductance Rate.In order to improve the reduction for the graphene oxide that electrical conductivity is carried out significantly decrease solubility (<0.5mg/mL) and cause Irreversible aggregation easily occurs for the material.According to the research from CNT, two kinds of main methods are investigated and have improved stone The surface nature of black alkene.First method be by the functionalisation of surfaces of as-reduced graphene oxide, it is solvable to manufacture Property, stable graphene is so that material is processed into possibility.For example, functional group's (for example ,-CH3 ,-SO3 group) passes through oxygen official (- O- ,-COOH) can be rolled into a ball to be connected on graphenic surface with covalent bond, but this method also can be in the sp2 conjugation of carbon atom Defect is introduced, this can influence intrinsic special performance such as high conductivity.Second method is using surfactant, polymer Or the non-covalent functionalization of aromatic molecules.Typically, good electrode material needs to meet some key requests:For electrolyte or The good wet effect of catalyst, the satisfactory electrical conductivity path in whole electrode material, and be quick diffusion and mass transport Required continuous poriferous network.So far, also it is not reaching to based on graphene using the effort of second method production material The theoretical performance of material.Instant invention overcomes these shortcomings be directed to optimize resin grapheme material preparation technology, prepare and Into resin graphene metallic composite, its electric property is excellent, electric conductivity is sensitive, has preferable application prospect.
The content of the invention
In order to solve the above technical problems, the present invention provides the preparation method of resin graphene metallic composite, the technique Graphene oxide solution is prepared using oxidation reaction, resin dispersion liquid is obtained using ultrasonic disperse microwave treatment, then passes through height Precision dc source carries out electro-deposition and obtains resin graphene metallic composite.The resin graphene metal composite being prepared Material, its electric property is excellent, electric conductivity is sensitive, has preferable application prospect.
The purpose of the present invention can be achieved through the following technical solutions:
The preparation method of resin graphene metallic composite, comprises the following steps:
(1) the 200mL concentrated sulfuric acids are added in dry beaker, are placed in ice-water bath, add 10g graphite under magnetic stirring With 7g sodium nitrate, it is sufficiently mixed, is then slowly added into 20g potassium permanganate, less than 10 DEG C are continued after stirring 2h, move into 35 DEG C Continue to stir 30min in tepidarium, 200mL distilled water is added dropwise, then heat to 90 DEG C, continue stirring reaction 30min, with distillation Reaction solution is diluted to 1000mL by water, then add 30g hydrogen peroxide, filter while hot, filter residue respectively with 5% hydrochloric acid and deionization Water washs repeatedly until aqueous ph value is 6.8-7.2, and dry in 45 DEG C of drying casees, grinding obtains graphite oxide powder after sieving End;
(2) the graphite oxide powder 2-6 parts for taking step (1) to obtain are placed in wide-mouth bottle, add what 100mL dewater treatments were crossed DMF, ultrasonic disperse obtain graphene oxide solution;
(3) by polytetrafluoroethylene (PTFE) 3-6 parts, polyether-ether-ketone 2-5 parts, polystyrene 1-3 parts, hydrogen peroxide 1-2 parts, dispersant After 1-2 parts are well mixed, deionized water 7-10 parts are added, are first ultrasonically treated successively, then at a temperature of 125-130 DEG C Microwave heating treatment 15-30min is carried out, is cooled to room temperature;
(4) resin dispersion liquid for obtaining graphene oxide solution obtained by step (2) and step (3), with metallic copper or silver Or anode electrode material of the iron as electro-deposition, using platinized platinum as the cathode electrode material of electro-deposition, by anode electrode material and Cathode electrode material is immersed in graphene/resin dispersion liquid electrodeposit liquid simultaneously, and electro-deposition is carried out using high precision DC power supply, Electro-deposition obtains graphene/resin metallic composite on anode electrode material surface after terminating;
(5) graphene obtained by step (4)/resin metallic composite is rinsed three times with 0.3% hydrochloric acid solution, Deionized water rinsing is used again three times, in 65 DEG C of drying, get product.
Preferably, the screen-aperture of 1000 mesh of ground screening in the step (1).
Preferably, the ultrasound condition in the step (2) and step (3) is 250KW, 30-60min.
Preferably, the dispersant in the step (3) is in atoleine, polyethylene glycol, magnesium stearate, Tissuemat E One or more.
Preferably, the high precision DC power supply in the step (4) applies constant voltage 2.0-2.5V progress electro-deposition, electricity Sedimentation time is 10 minutes.
Preferably, the distance between the anode electrode material in the step (4) and cathode electrode material are 5cm.
Compared with prior art, its advantage is the present invention:
(1) preparation method of resin graphene metallic composite of the invention prepares graphene oxide using oxidation reaction Solution, resin dispersion liquid is obtained using ultrasonic disperse microwave treatment, then carrying out electro-deposition by high precision DC power supply obtains Resin graphene metallic composite.The resin graphene metallic composite being prepared, its electric property is excellent, electric conductivity Can be sensitive, there is preferable application prospect.
(2) resin graphene metallic composite raw material of the invention be easy to get, technique it is simple, transported suitable for heavy industrialization With practical.
Embodiment
The technical scheme of invention is described in detail with reference to specific embodiment.
Embodiment 1
(1) the 200mL concentrated sulfuric acids are added in dry beaker, are placed in ice-water bath, add 10g graphite under magnetic stirring With 7g sodium nitrate, it is sufficiently mixed, is then slowly added into 20g potassium permanganate, less than 10 DEG C are continued after stirring 2h, move into 35 DEG C Continue to stir 30min in tepidarium, 200mL distilled water is added dropwise, then heat to 90 DEG C, continue stirring reaction 30min, with distillation Reaction solution is diluted to 1000mL by water, then add 30g hydrogen peroxide, filter while hot, filter residue respectively with 5% hydrochloric acid and deionization Water washs repeatedly until aqueous ph value is to be dried in 6.8,45 DEG C of drying casees, and grinding obtains graphite oxide powder, mistake after sieving The screen-aperture of 1000 mesh of screening;
(2) 2 parts of graphite oxide powder for taking step (1) to obtain is placed in wide-mouth bottle, adds the N that 100mL dewater treatments are crossed, Dinethylformamide, ultrasonic disperse obtain graphene oxide solution, ultrasound condition 250KW, 30min;
(3) it is 3 parts of polytetrafluoroethylene (PTFE), 2 parts of polyether-ether-ketone, 1 part of polystyrene, 1 part of hydrogen peroxide, 1 part of atoleine is mixed After closing uniformly, 7 parts of deionized water is added, is first ultrasonically treated successively, ultrasound condition 250KW, 30min, then 125 Microwave heating treatment 15min is carried out at a temperature of DEG C, is cooled to room temperature;
(4) resin dispersion liquid for obtaining graphene oxide solution obtained by step (2) and step (3), with metallic copper or silver Or anode electrode material of the iron as electro-deposition, using platinized platinum as the cathode electrode material of electro-deposition, by anode electrode material and Cathode electrode material immerses in graphene/resin dispersion liquid electrodeposit liquid simultaneously, anode electrode material and cathode electrode material it Between distance be 5cm, electro-deposition is carried out using high precision DC power supply, applies constant voltage 2.0V and carries out electro-deposition, electro-deposition Time is 10 minutes, and electro-deposition obtains graphene/resin metallic composite on anode electrode material surface after terminating;
(5) graphene obtained by step (4)/resin metallic composite is rinsed three times with 0.3% hydrochloric acid solution, Deionized water rinsing is used again three times, in 65 DEG C of drying, get product.
The performance test results of obtained resin graphene metallic composite are as shown in table 1.
Embodiment 2
(1) the 200mL concentrated sulfuric acids are added in dry beaker, are placed in ice-water bath, add 10g graphite under magnetic stirring With 7g sodium nitrate, it is sufficiently mixed, is then slowly added into 20g potassium permanganate, less than 10 DEG C are continued after stirring 2h, move into 35 DEG C Continue to stir 30min in tepidarium, 200mL distilled water is added dropwise, then heat to 90 DEG C, continue stirring reaction 30min, with distillation Reaction solution is diluted to 1000mL by water, then add 30g hydrogen peroxide, filter while hot, filter residue respectively with 5% hydrochloric acid and deionization Water washs repeatedly until aqueous ph value is to be dried in 6.9,45 DEG C of drying casees, and grinding obtains graphite oxide powder, mistake after sieving The screen-aperture of 1000 mesh of screening;
(2) 3 parts of graphite oxide powder for taking step (1) to obtain is placed in wide-mouth bottle, adds the N that 100mL dewater treatments are crossed, Dinethylformamide, ultrasonic disperse obtain graphene oxide solution, ultrasound condition 250KW, 40min;
(3) it is 4 parts of polytetrafluoroethylene (PTFE), 3 parts of polyether-ether-ketone, 1 part of polystyrene, 1 part of hydrogen peroxide, 1 part of polyethylene glycol is mixed After closing uniformly, 8 parts of deionized water is added, is first ultrasonically treated successively, ultrasound condition 250KW, 40min, then 125 Microwave heating treatment 20min is carried out at a temperature of DEG C, is cooled to room temperature;
(4) resin dispersion liquid for obtaining graphene oxide solution obtained by step (2) and step (3), with metallic copper or silver Or anode electrode material of the iron as electro-deposition, using platinized platinum as the cathode electrode material of electro-deposition, by anode electrode material and Cathode electrode material immerses in graphene/resin dispersion liquid electrodeposit liquid simultaneously, anode electrode material and cathode electrode material it Between distance be 5cm, electro-deposition is carried out using high precision DC power supply, applies constant voltage 2.0V and carries out electro-deposition, electro-deposition Time is 10 minutes, and electro-deposition obtains graphene/resin metallic composite on anode electrode material surface after terminating;
(5) graphene obtained by step (4)/resin metallic composite is rinsed three times with 0.3% hydrochloric acid solution, Deionized water rinsing is used again three times, in 65 DEG C of drying, get product.
The performance test results of obtained resin graphene metallic composite are as shown in table 1.
Embodiment 3
(1) the 200mL concentrated sulfuric acids are added in dry beaker, are placed in ice-water bath, add 10g graphite under magnetic stirring With 7g sodium nitrate, it is sufficiently mixed, is then slowly added into 20g potassium permanganate, less than 10 DEG C are continued after stirring 2h, move into 35 DEG C Continue to stir 30min in tepidarium, 200mL distilled water is added dropwise, then heat to 90 DEG C, continue stirring reaction 30min, with distillation Reaction solution is diluted to 1000mL by water, then add 30g hydrogen peroxide, filter while hot, filter residue respectively with 5% hydrochloric acid and deionization Water washs repeatedly until aqueous ph value is to be dried in 7.0,45 DEG C of drying casees, and grinding obtains graphite oxide powder, mistake after sieving The screen-aperture of 1000 mesh of screening;
(2) 4 parts of graphite oxide powder for taking step (1) to obtain is placed in wide-mouth bottle, adds the N that 100mL dewater treatments are crossed, Dinethylformamide, ultrasonic disperse obtain graphene oxide solution, ultrasound condition 250KW, 50min;
(3) it is 5 parts of polytetrafluoroethylene (PTFE), 4 parts of polyether-ether-ketone, 2 parts of polystyrene, 2 parts of hydrogen peroxide, 2 parts of magnesium stearate is mixed After closing uniformly, 9 parts of deionized water is added, is first ultrasonically treated successively, ultrasound condition 250KW, 50min, then 130 Microwave heating treatment 25min is carried out at a temperature of DEG C, is cooled to room temperature;
(4) resin dispersion liquid for obtaining graphene oxide solution obtained by step (2) and step (3), with metallic copper or silver Or anode electrode material of the iron as electro-deposition, using platinized platinum as the cathode electrode material of electro-deposition, by anode electrode material and Cathode electrode material immerses in graphene/resin dispersion liquid electrodeposit liquid simultaneously, anode electrode material and cathode electrode material it Between distance be 5cm, electro-deposition is carried out using high precision DC power supply, applies constant voltage 2.5V and carries out electro-deposition, electro-deposition Time is 10 minutes, and electro-deposition obtains graphene/resin metallic composite on anode electrode material surface after terminating;
(5) graphene obtained by step (4)/resin metallic composite is rinsed three times with 0.3% hydrochloric acid solution, Deionized water rinsing is used again three times, in 65 DEG C of drying, get product.
The performance test results of obtained resin graphene metallic composite are as shown in table 1.
Embodiment 4
(1) the 200mL concentrated sulfuric acids are added in dry beaker, are placed in ice-water bath, add 10g graphite under magnetic stirring With 7g sodium nitrate, it is sufficiently mixed, is then slowly added into 20g potassium permanganate, less than 10 DEG C are continued after stirring 2h, move into 35 DEG C Continue to stir 30min in tepidarium, 200mL distilled water is added dropwise, then heat to 90 DEG C, continue stirring reaction 30min, with distillation Reaction solution is diluted to 1000mL by water, then add 30g hydrogen peroxide, filter while hot, filter residue respectively with 5% hydrochloric acid and deionization Water washs repeatedly until aqueous ph value is to be dried in 7.2,45 DEG C of drying casees, and grinding obtains graphite oxide powder, mistake after sieving The screen-aperture of 1000 mesh of screening;
(2) 6 parts of graphite oxide powder for taking step (1) to obtain is placed in wide-mouth bottle, adds the N that 100mL dewater treatments are crossed, Dinethylformamide, ultrasonic disperse obtain graphene oxide solution, ultrasound condition 250KW, 60min;
(3) it is 6 parts of polytetrafluoroethylene (PTFE), 5 parts of polyether-ether-ketone, 3 parts of polystyrene, 2 parts of hydrogen peroxide, 2 parts of Tissuemat E is mixed After closing uniformly, 10 parts of deionized water is added, is first ultrasonically treated successively, ultrasound condition 250KW, 60min, Ran Hou Microwave heating treatment 30min is carried out at a temperature of 130 DEG C, is cooled to room temperature;
(4) resin dispersion liquid for obtaining graphene oxide solution obtained by step (2) and step (3), with metallic copper or silver Or anode electrode material of the iron as electro-deposition, using platinized platinum as the cathode electrode material of electro-deposition, by anode electrode material and Cathode electrode material immerses in graphene/resin dispersion liquid electrodeposit liquid simultaneously, anode electrode material and cathode electrode material it Between distance be 5cm, electro-deposition is carried out using high precision DC power supply, applies constant voltage 2.5V and carries out electro-deposition, electro-deposition Time is 10 minutes, and electro-deposition obtains graphene/resin metallic composite on anode electrode material surface after terminating;
(5) graphene obtained by step (4)/resin metallic composite is rinsed three times with 0.3% hydrochloric acid solution, Deionized water rinsing is used again three times, in 65 DEG C of drying, get product.
The performance test results of obtained resin graphene metallic composite are as shown in table 1.
Comparative example 1
(1) the 200mL concentrated sulfuric acids are added in dry beaker, are placed in ice-water bath, add 10g graphite under magnetic stirring With 7g sodium nitrate, it is sufficiently mixed, is then slowly added into 20g potassium permanganate, less than 10 DEG C are continued after stirring 2h, move into 35 DEG C Continue to stir 30min in tepidarium, 200mL distilled water is added dropwise, then heat to 90 DEG C, continue stirring reaction 30min, with distillation Reaction solution is diluted to 1000mL by water, then add 30g hydrogen peroxide, filter while hot, filter residue respectively with 5% hydrochloric acid and deionization Water washs repeatedly until aqueous ph value is to be dried in 6.8,45 DEG C of drying casees, and grinding obtains graphite oxide powder, mistake after sieving The screen-aperture of 1000 mesh of screening;
(2) it is 3 parts of polytetrafluoroethylene (PTFE), 2 parts of polyether-ether-ketone, 1 part of polystyrene, 1 part of hydrogen peroxide, 1 part of atoleine is mixed After closing uniformly, 7 parts of deionized water is added, is first ultrasonically treated successively, ultrasound condition 250KW, 30min, then 125 Microwave heating treatment 15min is carried out at a temperature of DEG C, is cooled to room temperature;
(3) resin dispersion liquid for obtaining graphene oxide solution obtained by step (1) and step (2), with metallic copper or silver Or anode electrode material of the iron as electro-deposition, using platinized platinum as the cathode electrode material of electro-deposition, by anode electrode material and Cathode electrode material immerses in graphene/resin dispersion liquid electrodeposit liquid simultaneously, anode electrode material and cathode electrode material it Between distance be 5cm, electro-deposition is carried out using high precision DC power supply, applies constant voltage 2.0V and carries out electro-deposition, electro-deposition Time is 10 minutes, and electro-deposition obtains graphene/resin metallic composite on anode electrode material surface after terminating;
(4) graphene obtained by step (3)/resin metallic composite is rinsed three times with 0.3% hydrochloric acid solution, Deionized water rinsing is used again three times, in 65 DEG C of drying, get product.
The performance test results of obtained resin graphene metallic composite are as shown in table 1.
Comparative example 2
(1) the 200mL concentrated sulfuric acids are added in dry beaker, are placed in ice-water bath, add 10g graphite under magnetic stirring With 7g sodium nitrate, it is sufficiently mixed, is then slowly added into 20g potassium permanganate, less than 10 DEG C are continued after stirring 2h, move into 35 DEG C Continue to stir 30min in tepidarium, 200mL distilled water is added dropwise, then heat to 90 DEG C, continue stirring reaction 30min, with distillation Reaction solution is diluted to 1000mL by water, then add 30g hydrogen peroxide, filter while hot, filter residue respectively with 5% hydrochloric acid and deionization Water washs repeatedly until aqueous ph value is to be dried in 7.2,45 DEG C of drying casees, and grinding obtains graphite oxide powder, mistake after sieving The screen-aperture of 1000 mesh of screening;
(2) 6 parts of graphite oxide powder for taking step (1) to obtain is placed in wide-mouth bottle, adds the N that 100mL dewater treatments are crossed, Dinethylformamide, ultrasonic disperse obtain graphene oxide solution, ultrasound condition 250KW, 60min;
(3) it is 6 parts of polytetrafluoroethylene (PTFE), 5 parts of polyether-ether-ketone, 3 parts of polystyrene, 2 parts of hydrogen peroxide, 2 parts of Tissuemat E is mixed After closing uniformly, 10 parts of deionized water is added, is ultrasonically treated, ultrasound condition 250KW, 60min, is cooled to room temperature;
(4) resin dispersion liquid for obtaining graphene oxide solution obtained by step (2) and step (3), with metallic copper or silver Or anode electrode material of the iron as electro-deposition, using platinized platinum as the cathode electrode material of electro-deposition, by anode electrode material and Cathode electrode material immerses in graphene/resin dispersion liquid electrodeposit liquid simultaneously, anode electrode material and cathode electrode material it Between distance be 5cm, electro-deposition is carried out using high precision DC power supply, applies constant voltage 2.5V and carries out electro-deposition, electro-deposition Time is 10 minutes, and electro-deposition obtains graphene/resin metallic composite on anode electrode material surface after terminating;
(5) graphene obtained by step (4)/resin metallic composite is rinsed three times with 0.3% hydrochloric acid solution, Deionized water rinsing is used again three times, in 65 DEG C of drying, get product.
The performance test results of obtained resin graphene metallic composite are as shown in table 1.
Embodiment 1-4 and comparative example 1-2 obtained resin graphene metallic composite is subjected to fracture toughness respectively This several value, dielectric constant, sheet resistance performance tests.
Table 1
It is molten that the preparation method of the resin graphene metallic composite of the present invention using oxidation reaction prepares graphene oxide Liquid, resin dispersion liquid is obtained using ultrasonic disperse microwave treatment, electro-deposition tree is then carried out by high precision DC power supply Fat graphene metallic composite.The resin graphene metallic composite being prepared, its electric property is excellent, electric conductivity It is sensitive, there is preferable application prospect.The resin graphene metallic composite raw material of the present invention is easy to get, technique is simple, is suitable to Heavy industrialization uses, practical.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair The equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks Domain, it is included within the scope of the present invention.

Claims (6)

1. the preparation method of resin graphene metallic composite, it is characterised in that comprise the following steps:
(1) the 200mL concentrated sulfuric acids are added in dry beaker, are placed in ice-water bath, add 10g graphite and 7g under magnetic stirring Sodium nitrate, it is sufficiently mixed, is then slowly added into 20g potassium permanganate, less than 10 DEG C are continued after stirring 2h, move into 35 DEG C of warm water Continue to stir 30min in bath, 200mL distilled water is added dropwise, then heat to 90 DEG C, continue stirring reaction 30min, will with distilled water Reaction solution is diluted to 1000mL, then adds 30g hydrogen peroxide, filters while hot, filter residue is anti-with 5% hydrochloric acid and deionized water respectively After backwashing is washed until aqueous ph value is 6.8-7.2, and dry in 45 DEG C of drying casees, grinding obtains graphite oxide powder after sieving;
(2) the graphite oxide powder 2-6 parts for taking step (1) to obtain are placed in wide-mouth bottle, add N, N- that 100mL dewater treatments are crossed Dimethylformamide, ultrasonic disperse obtain graphene oxide solution;
(3) by polytetrafluoroethylene (PTFE) 3-6 parts, polyether-ether-ketone 2-5 parts, polystyrene 1-3 parts, hydrogen peroxide 1-2 parts, dispersant 1-2 After part is well mixed, deionized water 7-10 parts are added, is first ultrasonically treated, then entered at a temperature of 125-130 DEG C successively Row microwave heating treatment 15-30min, is cooled to room temperature;
(4) resin dispersion liquid for obtaining graphene oxide solution obtained by step (2) and step (3), with metallic copper or silver or iron As the anode electrode material of electro-deposition, using platinized platinum as the cathode electrode material of electro-deposition, by anode electrode material and negative electrode Electrode material immerses in graphene/resin dispersion liquid electrodeposit liquid simultaneously, carries out electro-deposition using high precision DC power supply, electricity is heavy Product obtains graphene/resin metallic composite on anode electrode material surface after terminating;
(5) graphene obtained by step (4)/resin metallic composite is rinsed three times with 0.3% hydrochloric acid solution, then used Deionized water rinsing three times, in 65 DEG C of drying, get product.
2. the preparation method of resin graphene metallic composite according to claim 1, it is characterised in that the step (1) screen-aperture of 1000 mesh of ground screening in.
3. the preparation method of resin graphene metallic composite according to claim 1, it is characterised in that the step (2) ultrasound condition and in step (3) is 250KW, 30-60min.
4. the preparation method of resin graphene metallic composite according to claim 1, it is characterised in that the step (3) one or more of the dispersant in atoleine, polyethylene glycol, magnesium stearate, Tissuemat E in.
5. the preparation method of resin graphene metallic composite according to claim 1, it is characterised in that the step (4) high precision DC power supply in applies constant voltage 2.0-2.5V and carries out electro-deposition, and electrodeposition time is 10 minutes.
6. the preparation method of resin graphene metallic composite according to claim 1, it is characterised in that the step (4) the distance between anode electrode material and cathode electrode material in are 5cm.
CN201710968900.9A 2017-10-18 2017-10-18 The preparation method of resin graphene metallic composite Active CN107742545B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710968900.9A CN107742545B (en) 2017-10-18 2017-10-18 The preparation method of resin graphene metallic composite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710968900.9A CN107742545B (en) 2017-10-18 2017-10-18 The preparation method of resin graphene metallic composite

Publications (2)

Publication Number Publication Date
CN107742545A true CN107742545A (en) 2018-02-27
CN107742545B CN107742545B (en) 2019-05-17

Family

ID=61237523

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710968900.9A Active CN107742545B (en) 2017-10-18 2017-10-18 The preparation method of resin graphene metallic composite

Country Status (1)

Country Link
CN (1) CN107742545B (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102173414A (en) * 2011-03-18 2011-09-07 中国地质大学(武汉) Method for preparing graphene oxide by chemical peeling
US20140113200A1 (en) * 2011-07-25 2014-04-24 Fraser Seymour Functionalized Carbon Electrode, Related Material, Process for Production, and Use Thereof
CN106700136A (en) * 2016-11-18 2017-05-24 武汉理工大学 Graphene/chitosan composite material and preparation method thereof
US9928967B2 (en) * 2015-08-17 2018-03-27 Research Cooperation Foundation Of Yeungnam University Three-dimensional composites of nickel cobalt oxide/ graphene on nickel foam for supercapacitor electrodes, and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102173414A (en) * 2011-03-18 2011-09-07 中国地质大学(武汉) Method for preparing graphene oxide by chemical peeling
US20140113200A1 (en) * 2011-07-25 2014-04-24 Fraser Seymour Functionalized Carbon Electrode, Related Material, Process for Production, and Use Thereof
US9928967B2 (en) * 2015-08-17 2018-03-27 Research Cooperation Foundation Of Yeungnam University Three-dimensional composites of nickel cobalt oxide/ graphene on nickel foam for supercapacitor electrodes, and preparation method thereof
CN106700136A (en) * 2016-11-18 2017-05-24 武汉理工大学 Graphene/chitosan composite material and preparation method thereof

Also Published As

Publication number Publication date
CN107742545B (en) 2019-05-17

Similar Documents

Publication Publication Date Title
Teng et al. Modification of Nafion membrane using fluorocarbon surfactant for all vanadium redox flow battery
CN105460917B (en) A kind of nitrogen-doped carbon nanometer pipe and preparation method with hierarchy
CN106987857B (en) Single-layer metal structure molybdenum disulfide/redox graphene complex and preparation method thereof
CN105983708A (en) Preparation method of graphene nanosilver composite material
WO2016138802A1 (en) Method for preparing biomass graphene by using cellulose as raw material
CN108624775A (en) A kind of the graphene enhancing Cu-base composites and preparation method of supported copper
CN105155253A (en) Method for preparing conductive fabric by electrochemical reduction of graphene oxide
CN108598498A (en) The graphite felt electrode and preparation method thereof of N doping redox graphene modification
Meng et al. Room‐temperature dielectric switchable nanocomposites
CN105788879A (en) Graphene film and continuous preparation method thereof
CN107017093A (en) A kind of sulfonated graphene/Ni (OH)2The Preparation method and use of composite
CN107556510A (en) A kind of preparation method of flexible sensor electrode
CN106915741A (en) The preparation method of improved graphene oxide
CN103966644A (en) Preparation method for graphene/macromolecule emulsion composite film material
CN104803376A (en) Efficient preparation process of graphene oxide nanosheets
CN112675924A (en) Method for activating electrocatalyst and MoS obtained by same2Activated electrocatalyst and application
CN108677048A (en) A kind of silver-based composite material of nitrogen-doped graphene and preparation method thereof
CN209210955U (en) High modulus carbon fiber surface processing device
CN107742545B (en) The preparation method of resin graphene metallic composite
CN109321932A (en) Graphene and the preparation method and application thereof
CN109161947A (en) High modulus carbon fiber surface treatment method and device and its application
CN103804706B (en) A kind of ordered graphene electric-conduction polyimide film and preparation method thereof
CN107243259A (en) A kind of composite conductive film and preparation method thereof
CN105254909B (en) A kind of preparation method of conductive nano laminated film
KR20150067975A (en) Manufacturing method of cathode of microbial fuel cell and cathode of microbial fuel cell manufactured by the same

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
TA01 Transfer of patent application right

Effective date of registration: 20190419

Address after: 528300 No. 10 Chengfeng Road, Daliang Gujian Village Committee, Shunde District, Foshan City, Guangdong Province

Applicant after: GUANGDONG LUHUA NEW MATERIAL TECHNOLOGY HOLDING CO.,LTD.

Address before: 528000 Foshan, Guangdong, Foshan, Chancheng, 13 South China Road, Foshan, National Torch Innovation and entrepreneurship Park, sixteen block, block C.

Applicant before: FOSHAN HUICHUANG ZHENGYUAN NEW MATERIAL TECHNOLOGY Co.,Ltd.

TA01 Transfer of patent application right
GR01 Patent grant
GR01 Patent grant
PP01 Preservation of patent right

Effective date of registration: 20220531

Granted publication date: 20190517

PP01 Preservation of patent right